Quantitative analysis of gamma-hydroxybutyrate at endogenous concentrations in hair using liquid chromatography tandem mass spectrometry.

A method capable of quantifying endogenous concentrations of gamma-hydroxybutyrate (GHB) in human head hair was developed and validated using liquid chromatography/mass spectrometry/mass spectrometry (LC/MS/MS). Hair was digested under alkaline conditions, and GHB was isolated using liquid-liquid extraction. LC/MS/MS was performed using atmospheric pressure chemical ionization in the negative mode, multiple reaction monitoring, and deuterated internal standard (GHB-D(6)). Linearity was observed between 0.1 and 100 ng/mg GHB (R(2) = 1.000). The limits of detection and quantitation in human hair were 0.2 and 0.4 ng/mg, respectively. Accuracy at 2 ng/mg and 10 ng/mg was determined to be 97% and 94%, and intra-assay CVs at these concentrations were 5.2% and 7.4% (n = 4). Beta-hydroxybutyrate (BHB), alpha-hydroxybutyrate, gamma-butyrolactone, and 1,4-butanediol did not produce an interference, and there was negligible ion suppression or enhancement from the matrix.

Quantitative analysis of carisoprodol and meprobamate in whole blood using benzylcarbamate and deuterated meprobamate as internal standards.

Carisoprodol and meprobamate are frequently encountered drugs in impaired driving casework. Deuterated internal standards, although preferred, were not available until recently. Earlier published studies report the use of a variety of non-deuterated internal standards, many of which lack the chemical and physical similarities that are desired for quantitative analysis. Carisoprodol and meprobamate were determined in whole blood using solid-phase extraction and gas chromatography-mass spectrometry with benzylcarbamate and meprobamate-d(7) as internal standards. When benzylcarbamate was used as internal standard, the linear ranges for carisoprodol and meprobamate were 0-20 mg/L and 0-40 mg/L, respectively. The linear range increased to 100 mg/L when meprobamate-d(7) was used. Limits of detection for carisoprodol and meprobamate were 0.2 and 0.4 mg/L, respectively, regardless of the internal standard selection. The limit of quantitation for both drugs using either internal standard was 0.4 mg/L. Accuracies using benzylcarbamate and meprobamate-d(7) were 100-106% and 91-100%, respectively. Corresponding values for precision indicated intra-assay coefficients of variation of 2.6-4.3% for benzylcarbamate and 1.0-2.3% for meprobamate-d(7). No carryover was evident at 100 mg/L, the highest concentration tested, and no interferences were observed. Results indicated that either benzylcarbamate or meprobamate-d(7) is a suitable internal standard for quantitative determination of carisoprodol or meprobamate from whole blood.

Forensic analysis of a single particle of partially burnt gunpowder by solid phase micro-extraction-gas chromatography-nitrogen phosphorus detector.

Solid phase micro-extraction (SPME) was adopted to extract organic gun shot residues (OGSRs) from a single particle of partially burnt gunpowder. The partially burnt particle samples were collected from gun shot residue (GSR) deposited near the target areas. OGSRs, such as diphenylamine (DPA), methyl centralite (MC), ethyl centralite (EC), from only one single particle of partially burnt gunpowder were successfully extracted by SPME and analyzed by a gas chromatography coupled to a nitrogen phosphorus detector (GC-NPD). The results confirmed that the new extraction procedure is capable of extracting trace amount of MC and EC as signature molecules for the identification of GSR. The method represents a solvent-free extraction as a complementary analytical procedure for the forensic analysis of GSR-related evidences. The new extraction scheme with the capability of analyzing single particle of partially burnt gunpowder can also be applied to the identification of explosive residues, such as in post-blast investigations of improvised explosive devices.

Quantitative determination of caffeine and alcohol in energy drinks and the potential to produce positive transdermal alcohol concentrations in human subjects.

The purpose of this study was to determine whether non-alcoholic energy drinks could result in positive "alcohol alerts" based on transdermal alcohol concentration (TAC) using a commercially available electrochemical monitoring device. Eleven energy drinks were quantitatively assayed for both ethanol and caffeine. Ethanol concentrations for all of the non-alcoholic energy drinks ranged in concentration from 0.03 to 0.230% (w/v) and caffeine content per 8-oz serving ranged from 65 to 126 mg. A total of 15 human subjects participated in the study. Subjects consumed between 6 and 8 energy drinks over an 8-h period. The SCRAM II monitoring device was used to determine TACs every 30 min before, during, and after the study. None of the subjects produced TAC readings that resulted in positive "alcohol alerts". TAC measurements for all subjects before, during and after the energy drink study period (16 h total) were <0.02% (w/v). Subjects in the study consumed a quantity of non-alcoholic energy drink that greatly exceeds what would be considered typical. Based on these results, it appears that energy drink consumption is an unlikely explanation for elevated TACs that might be identified as potential drinking episodes or "alcohol alerts" using this device.